This research involved synthesizing In2S3–In(OH)3 nanosheets through a simple hydrothermal method at a low reaction temperature. The impact of different indium chloride concentrations on the morphology and crystal structure of In2S3–In(OH)3 nanostructures was investigated. The discussion extended to the photocatalytic hydrogen evolution of both In2S3–In(OH)3 nanosheets and nanofibers. These findings indicated that In2S3–In(OH)3 nanofibers exhibited optimal photocatalytic hydrogen production at various indium chloride concentrations. Furthermore, In2S3–In(OH)3–ZnS heterostructures were created by reacting In2S3–In(OH)3 nanosheets with varying concentrations of ZnS precursors. The study delved into the morphology and crystal structure, emphasizing photocatalytic hydrogen production in In2S3–In(OH)3–ZnS nanofibers under different concentrations of ZnS precursors. Remarkably, the In2S3–In(OH)3–ZnS nanofibers demonstrated exceptional hydrogen production efficiency, attributed to their larger specific surface area, improved blue light absorption, and reduced electron-hole pair recombination. Additionally, a comprehensive analysis explored the photocatalytic reaction mechanism, pH values, sacrificial reagents, sacrificial reagent concentrations, light source types, and intensities. These results highlighted the exceptional reusability of In2S3–In(OH)3–ZnS nanofibers in photocatalytic hydrogen production, showcasing their potential for cost-effective and highly efficient applications in diverse fields.
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